A method for preparing micro-nano KSrPO4 powder material at low temperature

Abstract

This invention provides a method for preparing micro / nano-sized KSrPO4 powder materials at low temperature, belonging to the field of inorganic non-metallic material preparation technology. Using K2CO3, SrCO3, and NH4H2PO4 as raw materials, KNO3 is mixed and ground with the above raw materials to obtain a precursor. The obtained precursor is calcined at 450-650℃ for 1-3 hours, and after cooling, a KSrPO4-salt mixture is obtained. The mixture is thoroughly washed multiple times with deionized water to remove the salt component, filtered, and dried to obtain micro / nano-sized KSrPO4 powder materials. The KSrPO4 material obtained by this invention has an average particle size of about 250 nm, with clear particle boundaries and good dispersibility. The method of this invention can reduce the preparation temperature, calcination time, and energy consumption; in addition, the preparation conditions are simple and controllable, and it is easy to achieve large-scale production.

Description

Technical Field

[0001] This invention belongs to the field of inorganic non-metallic material preparation technology, and specifically relates to a method for preparing micro-nano-scale KSrPO4 powder materials at low temperature. Background Technology

[0002] Currently, research on micron- and nano-scale materials is progressing rapidly both domestically and internationally. Nanomaterials, due to their unique surface effects, quantum size effects, macroscopic quantum tunneling effects, and volume effects, as well as their remarkable properties in catalysis, magnetism, electricity, optics, thermality, and chemical activity, have attracted widespread attention from materials scientists. Similarly, micro- and nanomaterials are widely used in various fields such as chemical engineering, environment, semiconductors, medicine, and agriculture due to their unique properties. For example, the unique internal structure and surface functional groups of carbon nanomaterials significantly improve their electrochemical performance; silver nanoparticles possess excellent antibacterial properties and have great potential in the development of antibacterial biomaterials; meanwhile, synthesized micron-structured Cu2O has also exhibited excellent visible-light photocatalytic degradation activity for organic pollutants; and embedding micro- and nano-rare earth compounds such as CeO2 into polymer materials can significantly improve the tensile strength of polymer materials.

[0003] KSrPO4 is composed of PO4 tetrahedrons embedded in KO 10 The long chains formed by polyhedra and SrO7 polyhedra are connected along the Z-axis, resulting in a complete three-dimensional crystal structure. This structure has applications in ceramics and luminescence, and is often used to synthesize fluorescent materials. Due to the unique physical and chemical properties of micro and nanomaterials, they are widely used in various fields. Therefore, preparing KSrPO4 materials with micro- and nano-sized particles can not only alter the material's physicochemical properties but also broaden its applications in other fields.

[0004] Currently, most domestic and international studies on the preparation of KSrPO4 materials employ solid-state methods. Typically, the raw materials are ball-milled for an extended period followed by high-temperature calcination to obtain KSrPO4 powder. This method results in KSrPO4 powder with high preparation temperatures and large particle sizes, exhibiting significant particle agglomeration. The literature "A new type of microwave dielectric ceramic based on K2O-SrO-P2O5 composition with high quality factor and low sintering temperature" requires ball milling for 24 hours followed by calcination at 950℃ for 3 hours to obtain the corresponding product. However, there are few reports on the low-temperature preparation of KSrPO4 materials with shorter preparation cycles. Therefore, researching the preparation of micro / nano-scale KSrPO4 powder materials under conditions of lower calcination temperatures and shorter calcination times has significant application value.

[0005] This invention employs a novel approach to prepare KSrPO4 materials. This method enables the KSrPO4 material to achieve micro-nano particle sizes with distinct particle boundaries and good dispersibility. It also boasts advantages such as low preparation temperature and short calcination time. Furthermore, the preparation conditions are controllable and the operation is simple, offering significant advantages for large-scale production. Therefore, this invention has considerable application value. Summary of the Invention

[0006] The purpose of this invention is to provide a method for preparing micro- and nano-sized KSrPO4 powder materials at low temperature. This method has the advantages of low preparation temperature, short preparation time, reduced energy consumption, simple preparation process, low process cost, and easy large-scale production. It can solve the problems of high preparation temperature, long preparation time, large particle size, and obvious agglomeration between particles in the current method.

[0007] The technical solution of this invention is as follows:

[0008] A method for preparing micro / nano-sized KSrPO4 powder materials at low temperature with an average particle size of 250 nm includes the following steps:

[0009] (1) K2CO3, SrCO3 and NH4H2PO4 were weighed as raw materials according to the molar ratio K2CO3:SrCO3:NH4H2PO4=1:2:2, and KNO3 was weighed and mixed with the above raw materials to obtain the precursor.

[0010] (2) The precursor obtained in step (1) is transferred to a muffle furnace and calcined in an air atmosphere. After the calcination time is over, it is cooled to obtain a KSrPO4-salt mixture.

[0011] (3) The mixture obtained in step (2) is washed thoroughly with deionized water multiple times to remove the salt components, and then filtered and dried to obtain micro-nano KSrPO4 powder.

[0012] In step (1), the molar ratio of K2CO3:SrCO3:NH4H2PO4:KNO3 is 1:2:2:(12-28).

[0013] In step (2), the calcination temperature is 450-650℃ and the calcination time is 1-3h.

[0014] The beneficial effects of this invention are:

[0015] (1) The present invention adopts a new preparation method to prepare KSrPO4 material at a low temperature of 450℃. Compared with the traditional solid-state method, this method can reduce the preparation temperature of the material and reduce energy consumption.

[0016] (2) The KSrPO4 material prepared by this invention has a particle size of micro-nano level, with an average of about 250nm, clear particle boundaries, and good dispersibility.

[0017] (3) The preparation conditions of this invention are controllable, the operation process is simple, the prepared material has high purity and the particle size is at the micro-nano level, and it is easy to achieve large-scale production. Attached Figure Description

[0018] Figure 1 The image shows the XRD pattern of the micro / nano-scale KSrPO4 powder material prepared in Example 1.

[0019] Figure 2 The XRD patterns of the micro / nano-scale KSrPO4 powder materials prepared in Examples 2 and 3 are shown below: a is the sample at 450℃ in Example 2, b is the sample at 500℃ in Example 2, c is the sample at 550℃ in Example 2, and d is the XRD pattern of Example 3.

[0020] Figure 3 The XRD patterns of the micro / nano-scale KSrPO4 powder materials prepared in Examples 4-7 are shown below: where a is the XRD pattern of Example 4, b is the XRD pattern of Example 5, c is the XRD pattern of Example 6, and d is the XRD pattern of Example 7.

[0021] Figure 4 The image shows a SEM image of the micro / nano-scale KSrPO4 powder material prepared in Example 1.

[0022] Figure 5SEM images of the micro / nano-scale KSrPO4 powder materials prepared in Examples 2 and 3: (a) is the sample at 450℃ in Example 2, (b) is the sample at 500℃ in Example 2, (c) is the sample at 550℃ in Example 2, and (d) is the SEM image of Example 3.

[0023] Figure 6 SEM images of the micro / nano-scale KSrPO4 powder materials prepared in Examples 4 and 5: (a) is an SEM image of Example 4 and (b) is an SEM image of Example 5.

[0024] Figure 7 SEM images of the micro / nano-scale KSrPO4 powder materials prepared in Examples 6 and 7: (a) is an SEM image of Example 6 and (b) is an SEM image of Example 7. Detailed Implementation

[0025] The specific embodiments of the present invention will be further described below with reference to the accompanying drawings and technical solutions.

[0026] Example 1:

[0027] Weigh out K2CO3 according to the molar ratio K2CO3:SrCO3:NH4H2PO4:KNO3 = 1:2:2:20. 3、 Using SrCO3 and NH4H2PO4 as raw materials, a corresponding amount of KNO3 was mixed and ground with the above raw materials for 25 min to obtain a precursor. The precursor was transferred to a muffle furnace and calcined in an air atmosphere at a temperature of 600℃ for 2 h. After the calcination time was over, the mixture was cooled to obtain a KSrPO4-salt mixture. The KSrPO4-salt mixture obtained above was thoroughly washed with deionized water several times to remove the salt components. After filtration, it was dried at 108℃ for 1.5 h to obtain micro-nano-scale KSrPO4 powder material.

[0028] Example 2:

[0029] The difference between this embodiment and Example 1 is that the calcination temperatures are 450, 500, and 550°C, respectively, and the specific preparation methods are as follows:

[0030] Weigh out K2CO3 according to the molar ratio K2CO3:SrCO3:NH4H2PO4:KNO3 = 1:2:2:20. 3、Using SrCO3 and NH4H2PO4 as raw materials, a corresponding amount of KNO3 was mixed and ground with the above raw materials for 25 min to obtain a precursor. The precursor was transferred to a muffle furnace and calcined in an air atmosphere at a temperature of 450℃ for 2 h. After the calcination time was over, the mixture was cooled to obtain a KSrPO4-salt mixture. The KSrPO4-salt mixture obtained above was thoroughly washed with deionized water several times to remove the salt components. After filtration, it was dried at 108℃ for 1.5 h to obtain micro-nano-scale KSrPO4 powder material.

[0031] The preparation steps were the same as above, except that the calcination temperatures were changed to 500 and 550℃ respectively, and two micro-nano-scale KSrPO4 powder materials were obtained.

[0032] Example 3:

[0033] The difference between this embodiment and Embodiments 1-2 is that the calcination temperature is 650℃, and the specific preparation method is as follows:

[0034] Weigh out K2CO3 according to the molar ratio K2CO3:SrCO3:NH4H2PO4:KNO3 = 1:2:2:20. 3、 Using SrCO3 and NH4H2PO4 as raw materials, a corresponding amount of KNO3 was added and mixed with the above raw materials and ground for 25 min to obtain a precursor. The precursor was transferred to a muffle furnace and calcined in an air atmosphere at a temperature of 650℃ for 2 h. After the calcination time was over, the mixture was cooled to obtain a KSrPO4-salt mixture. The obtained KSrPO4-salt mixture was thoroughly washed with deionized water several times to remove the salt components. After filtration, it was dried at 108℃ for 1.5 h to obtain micro-nano-scale KSrPO4 powder material.

[0035] Example 4:

[0036] The difference between this embodiment and embodiments 1-3 is that the calcination time is 1 hour, and the specific preparation method is as follows:

[0037] Weigh out K2CO3 according to the molar ratio K2CO3:SrCO3:NH4H2PO4:KNO3 = 1:2:2:20. 3、 Using SrCO3 and NH4H2PO4 as raw materials, a corresponding amount of KNO3 was mixed and ground with the above raw materials for 25 min to obtain a precursor. The precursor was transferred to a muffle furnace and calcined in an air atmosphere at a temperature of 600℃ for 1 h. After the calcination time was over, the mixture was cooled to obtain a KSrPO4-salt mixture. The KSrPO4-salt mixture obtained above was thoroughly washed with deionized water several times to remove the salt components. After filtration, it was dried at 108℃ for 1.5 h to obtain micro-nano-scale KSrPO4 powder material.

[0038] Example 5:

[0039] The difference between this embodiment and embodiments 1-4 is that the calcination time is 3 hours, and the specific preparation method is as follows:

[0040] Weigh out K2CO3 according to the molar ratio K2CO3:SrCO3:NH4H2PO4:KNO3 = 1:2:2:20. 3、 Using SrCO3 and NH4H2PO4 as raw materials, a corresponding amount of KNO3 was mixed and ground with the above raw materials for 25 min to obtain a precursor. The precursor was transferred to a muffle furnace and calcined in an air atmosphere at a temperature of 600℃ for 3 h. After the calcination time was over, the mixture was cooled to obtain a KSrPO4-salt mixture. The KSrPO4-salt mixture obtained above was thoroughly washed with deionized water several times to remove the salt components. After filtration, it was dried at 108℃ for 1.5 h to obtain micro-nano-scale KSrPO4 powder material.

[0041] Example 6:

[0042] The difference between this embodiment and Examples 1-5 is that the molar ratio of the raw materials is K2CO3:SrCO3:NH4H2PO4:KNO3 = 1:2:2:12, and the specific preparation method is as follows:

[0043] Weigh out K2CO3 according to the molar ratio K2CO3:SrCO3:NH4H2PO4:KNO3 = 1:2:2:12. 3、 Using SrCO3 and NH4H2PO4 as raw materials, a corresponding amount of KNO3 was mixed and ground with the above raw materials for 25 min to obtain a precursor. The precursor was transferred to a muffle furnace and calcined in an air atmosphere at a temperature of 600℃ for 2 h. After the calcination time was over, the mixture was cooled to obtain a KSrPO4-salt mixture. The KSrPO4-salt mixture obtained above was thoroughly washed with deionized water several times to remove the salt components. After filtration, it was dried at 108℃ for 1.5 h to obtain micro-nano-scale KSrPO4 powder material.

[0044] Example 7:

[0045] The difference between this embodiment and Examples 1-6 is that the molar ratio of the raw materials is K2CO3:SrCO3:NH4H2PO4:KNO3 = 1:2:2:28, and the specific preparation method is as follows:

[0046] Weigh out K2CO3 according to the molar ratio K2CO3:SrCO3:NH4H2PO4:KNO3 = 1:2:2:28. 3、Using SrCO3 and NH4H2PO4 as raw materials, a corresponding amount of KNO3 was mixed and ground with the above raw materials for 25 min to obtain a precursor. The precursor was transferred to a muffle furnace and calcined in an air atmosphere at a temperature of 600℃ for 2 h. After the calcination time was over, the mixture was cooled to obtain a KSrPO4-salt mixture. The KSrPO4-salt mixture obtained above was thoroughly washed with deionized water several times to remove the salt components. After filtration, it was dried at 108℃ for 1.5 h to obtain micro-nano-scale KSrPO4 powder material.

[0047] Figure 1-3 The XRD patterns of the KSrPO4 materials prepared in Examples 1-7 are shown. As can be seen from the XRD patterns, the diffraction peaks are high, indicating that the present invention can prepare KSrPO4 materials with high crystallinity.

[0048] Figure 4-7 The images show SEM images of the KSrPO4 materials prepared in Examples 1-7. As can be seen from the SEM images, micro-nano-scale KSrPO4 powder materials were obtained, with an average particle size of about 250 nm, clear particle boundaries, and good dispersibility.

[0049] The above description illustrates and illustrates the basic principles and main features of the present invention. However, the above description is only a specific embodiment of the present invention. The technical features of the present invention are not limited thereto. All changes and modifications made in accordance with the scope of the patent application of the present invention should be included in the scope of the present invention.

Claims

1. A method for preparing micro / nano-scale KSrPO4 powder materials at low temperature, comprising the following steps: (1) Weigh K2CO3, SrCO3 and NH4H2PO4 as raw materials, and weigh KNO3 and mix and grind them with the above raw materials to obtain a precursor; (2) The precursor obtained in step (1) is transferred to a muffle furnace and calcined in an air atmosphere. After the calcination time is over, it is cooled to obtain a KSrPO4-salt mixture. (3) The mixture obtained in step (2) is thoroughly washed multiple times with deionized water to remove the salt components, and then filtered and dried to obtain micro-nano-sized KSrPO4 powder; characterized in that, In step (1), the molar ratio of K2CO3, SrCO3, NH4H2PO4 and KNO3 is 1:2:2:(12-28); in step (2), the calcination temperature is 450-650ºC and the calcination time is 1-3h.

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